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Preparation of sulfydryl graphene modified electrode and trace heavy metal detection method thereof

A fossil and graphene technology, applied in the preparation of thiolated graphene-modified electrodes and the detection of trace heavy metals, can solve the problems of difficult storage of biomolecules, unsuitable for rapid detection, expensive instruments, etc., to facilitate adsorption and enrichment , many surface active sites, good stability and reproducibility

Active Publication Date: 2014-03-26
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Atomic absorption spectrometry is an important method for detecting heavy metals, widely used in environmental monitoring, but requires corresponding element lamps during the detection process, and is not suitable for on-site rapid detection
The inductively coupled plasma method can be used for trace detection, but the instrument is expensive, the detection speed is slow, the continuity is poor, and the environmental requirements are high
Biochemical methods have good specificity, but poor repeatability, and biomolecules are difficult to preserve

Method used

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  • Preparation of sulfydryl graphene modified electrode and trace heavy metal detection method thereof
  • Preparation of sulfydryl graphene modified electrode and trace heavy metal detection method thereof
  • Preparation of sulfydryl graphene modified electrode and trace heavy metal detection method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Electrode preparation process

[0035] (1) Preparation of thiol-functionalized graphene-modified electrodes

[0036] a. First prepare graphene oxide by the Hummer method, then take 500mg graphene oxide and place it in a round bottom flask, add 500mg sodium hydroxide and 100mL water, reflux at 70°C for 1h after ultrasonic dispersion, wait for the solution to cool, centrifuge and wash To neutral, vacuum dry. 200 mg of the prepared alkali-treated graphene oxide was ultrasonically dispersed in 100 mL of aqueous solution, 5 g of bromoacetic acid and 6 g of sodium hydroxide were added for ultrasonic reaction for 3 h, centrifuged, washed until neutral, and dried to obtain carboxylated graphene oxide. Then take 100 mg of carboxylated graphene oxide and disperse it in 100 mL of water, add 1.5 mL of hydrazine hydrate, react at 95°C for 1 hour, centrifuge, wash and dry to obtain carboxylated graphene.

[0037] b Take 50 mg of carboxylated graphene and disperse it in a 100 mL fla...

Embodiment 2

[0048] Electrode preparation process

[0049] (1) Preparation of thiol-functionalized graphene-modified electrodes

[0050] The preparation method is the same as that of Example 1.

[0051] (2) Ultrasonic disperse the mercapto-functionalized graphene into a 0.2 mg / mL dispersion.

[0052] (3) Take 15 μL of the dispersion liquid and apply it on the surface of the glassy carbon electrode polished to a mirror surface. The diameter of the glassy carbon electrode is 4mm, and let it dry naturally to make a working electrode.

[0053] Detection process

[0054] (1) Test bottom fluid

[0055] Phosphate buffer solution was selected as the test base solution, and the pH of the solution was 5.0;

[0056] (2) Enrichment

[0057] Enrichment potential selection -1.2V, deposition time 100s, equilibration time 10s;

[0058] (3) Dissolution

[0059] Using differential pulse stripping voltammetry, set initial potential -1.0, end potential -0.2, potential increment 0.0002V, pulse amplitude...

Embodiment 3

[0061] Electrode preparation process

[0062](1) Preparation of thiol-functionalized graphene-modified electrodes

[0063] a. First, use the Hummer method to prepare graphene oxide, then take 500mg graphene oxide and place it in a round bottom flask, add 500mg sodium hydroxide and 100mL water, reflux at 70°C for 1h after ultrasonic dispersion, wait for the solution to cool, and centrifuge, Wash until neutral and dry in vacuum. The obtained alkali-treated graphene oxide was ultrasonically dispersed to form 100 mL of a 2 g / L aqueous solution, and 5 g of bromoacetic acid and 6 g of sodium hydroxide were added for ultrasonic reaction for 3 hours. The product was centrifuged, washed, and vacuum-dried to obtain carboxylated graphene oxide. Then, take 100 mg of carboxylated graphene oxide and disperse it in 100 mL of water, add 1.5 mL of hydrazine hydrate, react at 95°C for 1 hour, centrifuge, wash and dry to obtain carboxylated graphene.

[0064] b. Take 50 mg of carboxylated grap...

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Abstract

The invention provides an electrochemical sensor detection method of trac heavy metal ions, and relates to a sulfydryl functionalized graphene modified glassy carbon electrode, and preparation and application of the electrode, and belongs to the technical field of heavy metal detection and electrochemical analysis. The method specifically comprises the following steps: modifying sulfydryl functionalized graphene on the surface of the glassy carbon electrode so as to manufacture a sensor, and detecting the trace heavy metal ions by using an electrochemical differential pulse stripping voltammetry method. The method can be directly applied to rapid electrochemical detection on the heavy metal ions, and has the advantages of high sensitivity, wide linearity range, low detection limit and the like.

Description

Technical field [0001] The invention relates to the technical fields of heavy metal detection and electrochemical analysis, and specifically to the preparation of a thiolated graphene modified electrode and a method for detecting trace amounts of heavy metals. Background technique [0002] With the rapid development of my country's economy, heavy metal pollution has become one of the increasingly serious environmental problems, attracting great attention from the whole society. Heavy metal pollution is concentrated and difficult to degrade in the environment. Cadmium among them can cause irritation to the respiratory tract, and long-term exposure can cause anosmia. Cadmium compounds are not easily absorbed by the intestines and accumulate in the liver or kidneys, causing harm. In severe cases, middle-age syndrome may occur. Toxic pulmonary edema leads to respiratory failure and death. In recent years, the frequent occurrence of heavy metal cadmium pollution incidents has so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/30G01N27/48
Inventor 王会才于璐洋赵修青马振华姚晓霞铁凝
Owner TIANJIN POLYTECHNIC UNIV
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